无负极锂金属电池的界面改性研究

锂金属兼具电位负（–3.04 V，相对标准氢电极）、比重轻（M=6.94 g mol^–1、r=0.534 g cm^–3）、半径小（76 pm）和容量大（3860 mAh g^–1）的特殊优点，成为理想的负极材料。然而，其高活性导致电沉积过程中锂成核不均匀、界面不稳定和体积膨胀等问题，从而引发不可控的锂枝晶生长。锂枝晶会诱导电解液持续分解和死锂产生，导致电池容量快速衰减，并引发电池短路和热失控等安全问题，限制了其商业化应用。本论文主要围绕调控负极表面的电子分布、固体电解质膜（SEI）的构造，构建聚合物人工SEI膜，以及优化固态电解质/电极界面的离子传输三个方面，深入探讨无锂铜负极在锂沉积/剥离过程中的成核、沉积行为、界面演变机制，以及对全电池的电化学性能影响机制。具体研究内容如下：

针对无负极锂金属电池中的不可控锂枝晶生长问题，通过精确设计亲锂三维多孔阵列集流体，诱导原位生成有序孤立梯度结构SEI膜，有效抑制锂枝晶生长和体积膨胀问题。采用纳米压印方法制备三维多孔阵列结构的铜集流体，并通过优化多孔结构调控金属锂沉积空间，从而抑制体积膨胀并释放局部应力。孔洞内壁修饰的CuCl经电化学锂化后，原位形成纳米铜成核位点和有序孤立且LiCl浓度梯度分布的SEI膜。亲锂纳米铜成核位点降低金属锂成核活化能，诱导金属锂在孔洞内优先沉积；SEI膜的独特构造赋予其高的机械稳定性和锂离子传导率，抑制锂枝晶生长，从而提升循环稳定性。亲锂三维多孔无锂铜负极与磷酸铁锂正极组装的全电池，库伦效率大于99.4%，放电容量大于130 mAh g^–1，100次循环后，容量保持率大于70%。有序孤立梯度SEI膜诱导金属锂稳定沉积为解决锂枝晶难题、推进可充金属锂电池的工业应用，提供了新思路。

针对无负极锂金属电池中普遍存在的界面不稳定等问题，通过在电极表面涂覆葡聚糖磺酸锂（LDS）粘结剂作为人工SEI膜，增强了电极界面层的粘结力、机械稳定性和锂离子电导率。利用LDS涂层改性的铜箔作为无锂铜负极（LDS-Cu），与钴酸锂正极组装的全电池，在碳酸酯和醚类电解液中均展现出较低的锂沉积过电位，及优异的循环稳定性。100次循环后全电池容量保持率超过72.1%，接近目前文献报道的无负极金属锂电池循环稳定性最佳值。这主要归因于LDS的高锂离子传导率，以及在碳酸酯和醚类电解液中溶胀率低。LDS分子主链上的聚糖苷结构，具有良好的柔性和机械互锁作用，赋予LDS涂层良好的弹性和机械稳定性；分子链上的磺酸官能团（-SO₃Li），具有优良的络合作用力，可以动态的与铜集流体及金属锂形成强的粘附力；同时，磺酸锂不仅离子传导率高、且具有单离子电导特性，有助于抑制浓差极化和副反应发生，进而优化了无锂负极倍率性能与库伦效率。功能化有机锂盐粘结剂通过涂覆成功改性电极界面，为解决锂枝晶和稳定电极/电解液界面提供了一个简单有效策略。

针对固态电池中固态电解质内部以及电极/固态电解质固固界面阻抗大等难题，充分利用界面稳定材料LDS的强粘合力和高离子传导率特性，复合Li_6.3La₃Zr_1.4Ta_0.6O₁₂ (LLZTO)无机快离子导体，制备复合固态电解质膜（LDS-LLZTO）。LDS作为界面稳定层，降低了LLZTO颗粒的固固界面以及正负极和复合电解质的固固界面阻抗。LDS-LLZTO与无锂多孔阵列铜负极、磷酸铁锂正极组装成一体化结构无负极全固态锂金属电池，在0.5C下的放电容量大于130 mAh g^–1，经100个循环后容量保留率仍高于68%。可归因于LDS-LLZTO复合固态电解质具有高弹性、高模量、锂离子迁移数大和高离子电导率（室温导离子率可达0.37 mS cm^–1）等特性，从而实现锂离子在铜箔上的均匀且可逆沉积。因此，葡聚糖磺酸锂作为固固界面稳定层材料，对设计高性能固态锂金属电池有重要的启发意义。

总之，本论文研究结果表明，三维集流体结合有序孤立梯度结构SEI膜可以有效抑制锂枝晶和死锂的生成，稳定金属锂沉积；葡聚糖磺酸锂作为界面改性材料，不仅可以作为人工SEI膜解决液态金属锂电池中负极界面稳定性问题，还可以有效稳定电极界面、固态电解质内部及其正负极之间的固固界面，降低界面阻抗，为开发高性能可充锂金属电池以及固态锂电池提供了新思路，对推动高能锂电池技术的发展有重要意义。

Lithium metal is generally considered as a most promising anode material due to its unique combination of a low redox electrochemical potential (−3.04 V vs. the standard hydrogen electrode), light weight (M=6.94 g mol⁻¹, ρ=0.534 g cm⁻³), small radius (76 pm), and high theoretical capacity (3860 mAh g⁻¹). However, the high reactivity of lithium metal also gives rise to many undesired problems, including non-uniform nucleation, interface instability, and volume expansion during electrodeposition. These would cause uncontrolled lithium dendrite formation, which would furtherly result in the persistent electrolyte depletion and the formation of dead lithium. These chain reactions would furtherly culminate in rapid capacity degradation, short circuits and thermal runaway, thereby hindering the commercialization of lithium metal batteries (LMBs). This thesis investigated the nucleation, deposition/stripping and interfacial evolution mechanisms of lithium metal on copper anodes from three aspects: interfacial electron regulation and reconstruction of solid electrolyte interphase (SEI), development of artificial polymer-based SEI layers, and optimization of ion transport within solid electrolyte/electrode interfaces. The main works in this thesis are briefly summarized as follows.

To address the challenge of uncontrolled lithium dendrite growth in anode-free LMBs, a lithiophilic three-dimensional (3D) porous current collector (CC) was precisely designed to induce the in-situ formation of gradient solid electrolyte interface (SEI) with ordered and isolated components, effectively suppressing lithium dendrite growth and volume expansion. The 3D porous structure on the copper CC surface was fabricated using nanoimprint lithography, and the optimized porous structure regulated metallic lithium deposition, suppressed volume expansion, and alleviated local stress. After the initial electrochemical lithiation of the CuCl-coated pore surface, an orderly isolated SEI film containing LiCl with concentration gradient, along with in situ-formed Cu nanoparticles, was generated. This structure subsequently facilitated the selective deposition of lithium within the interior of the pores. The lithiophilic Cu nanoparticles as nucleation sites reduced the nucleation activation energy of metallic lithium. The in-situ formed SEI not only exhibited high lithium-ion conductivity, but also effectively inhibited the lithium dendrite growth and dead lithium formation during lithium deposition, thereby significantly enhancing the mechanical and cycling stability of the anode-free system. Through assembling full cells with the modified copper CC as anode and the LiFePO₄ as cathode, it achieved a Coulombic efficiency exceeding 99.4%, a discharge capacity surpassing 130 mAh g^–1, and a capacity retention ratio above 70% after 100 cycles. This approach offers a novel solution to the lithium dendrite issue, paving the way for the industrial application of rechargeable anode-free LMBs.

To address the prevalent issues of interfacial instability in anode-free LMBs, lithium dextran sulfate (LDS), a binder, was employed as an artificial SEI film, which contributed to enhancing the adhesion, mechanical stability, and lithium-ion conductivity at the electrode interface. The full cell, assembled with LDS-coated copper foil (LDS-Cu) as a lithium-free anode and a LiCoO₂ cathode, exhibited low lithium deposition overpotential and excellent cycling stability in both carbonate and ether-based electrolytes. The capacity retention rate surpasses 72.1% after 100 cycles, approaching the best reported values for anode-free LMBs in the literature. This can be primarily attributed to the high ionic conductivity and low swelling rate of the LDS protective layer in electrolytes. Specifically, the glycosidic structure in the LDS molecular chain endowed themselves with flexibility and mechanical interlocking properties, which contributed to creating a LDS coating layer with excellent elasticity and mechanical stability on the CC. The sulfonic acid functional groups (-SO₃Li) on the molecular chain can reversibly, dynamically, and strongly bind to the copper CCs as well as metallic Li. Furthermore, the high lithium-ion conductivity and single-ion conduction characteristics of lithium sulfonate contributed to suppressing concentration polarization and side reactions, thereby optimizing the rate performance and Coulombic efficiency of the lithium-free anode. The functionalized organic lithium salt binder coating provides a simple and effective strategy for suppressing lithium dendrite formation and stabilizing the electrode/electrolyte interface.

To address the challenges of high internal and electrode/solid electrolyte interfacial impedance in solid-state LMBs, a novel composite solid-state electrolyte was fabricated by exploiting the exceptional adhesive strength and high ionic conductivity of functionalized LDS in combination with Li_6.3La₃Zr_1.4Ta_0.6O₁₂ (LLZTO) inorganic fast-ion conductor. Serving as an interfacial stabilizing layer, LDS effectively mitigated the solid-solid interface impedance between the different LLZTO particles as well as the anode/cathode and the LDS-LLZTO composite electrolyte. The full cell assembled with lithium-free porous copper anode, LDS-LLZTO and LiFePO₄ cathode, exhibited a discharge capacity exceeding 130 mAh g^–1 at 0.5C and maintained over 68% capacity retention following 100 cycles. The superior performance of the battery can be attributed to the exceptional properties of the LDS-LLZTO composite solid-state electrolyte, including notable elasticity, high modulus, substantial lithium-ion transference number, and impressive ionic conductivity (0.37 mS cm^–1 at room temperature). These factors synergistically contribute to the stabilization of uniform and reversible lithium deposition on the copper foil. Consequently, LDS's role as a solid-solid interface stabilizing material offers valuable guidance in devising high-performance solid-state LMBs.

In summary, the findings in this thesis indicated that incorporating a 3D CC with an orderly isolated gradient structure SEI film can effectively suppress the formation of lithium dendrites and dead lithium, thereby stabilizing lithium deposition. LDS not only can act as an artificial SEI to enable the stability of SEI for Li metal anode, but also as an interfacial modification material, which can efficiently stabilize the solid-solid interface within the solid electrolyte and between the anode and cathode, therefore reducing the interfacial impedance. These findings offer fresh perspectives for the development of high-performance rechargeable LMBs and all-solid-state lithium batteries, which are of great significance in driving forward lithium battery technology advancements.

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